Method of refining rosin



Patented Apr. 14, 1931 UNITED STATES IBVDI' W. 3mm, 0] WHAB'ION, NEW JERSEY, ASSIGNOB 1'0 PAT ENT OFFICE POWDEB IE'I'EOD OI ammo 308111 In Drawing. Application filed August 28, 1928, serial Io. 181,138. Renewed August 15, 198.

My invention relates to a process of treating rosin, both wood. rosin, which, while marketable; is of a low grade, and the lower ades of rosin, so as to remove therein practically all of the objectionable coloring matter and produce a high grade rosin adapted for use insizing the higher grades of paper and in the manufacture of the better grades of varnish and which is so thorurified and refined that it is ada ted or use in the manufacture of high gra e rosin soaps vand limed varnishes of satisfactory color, as well as for most, if not all, other purposes to which the high grade gum rosin is adapted.

The rosin tobe purified by my process may be produced as such from either wood or gum rosins by any of the usual and well known processes, or it may be purified as found in drop liquor}; which, as is well from which turpentine has been removed by steam, with gasoline, and which contains chiefly rosin, pine oil and various coloring es. In carrying out the process embodying my invention, the rosin, especially wood rosin,

A may be subjected to any desired prelimi- 'n distillation process or the rosin may be dis phenol (0 H, H)" which though it has a dered meltin point of a out 40 C. maybe rendiquid by the addition of a small amount of water, it having been discovered by me that phenol has the capacity for selectively dissolving out the color bodies from Typical of the practice of'my invention usin .Puri

rdinary phenol C H OH), as the g agent, the following treatment of wood rosin will be illustrative Wood rosin, produced by any of the known processes, is dissolved in a suitable solvent, for example, gasoline, to form a oding wood stock,

rosin solution containing say about 15%, by weight, of rosin to which is added phenol. For example, say 800 g. of gasoline-rosin solution, containing 15% rosin is extracted with a mixture of 250 g. of phenol and 40 u g. of water. A

The rosin solution and phenol and water should be thoroughly mixed and then allowed to separate into two layers, one of which is primarily phenol, water and extracted color bodies, with a small proportion of the rosin, and the other'of which is primarily gasoline and purified rosin, with a small amount of phenol. somewhat soluble in the gasoline-rosin solution at certain temperatures, its solubility decreasing with reduction of temperature below normal atmospheric tem Therefore, separation may be .facihtated and made more complete by effecting the separation into layers at a reduced temperature, sa a temperature of about 7 C.

he" gasoline-rosin solution is separated from the phenol solution by any convenient method, as by gravity or centrifugal force."

Since the phenol is to some extent soluble in the asoline at the suggested temperature of 7 the gasoline-rosin solution is preferably washed with water or dilute aqueous alkali solution in order to remove from it the so small amount of phenolwhich it contains. The purified rosin may now be recovered from the gasoline-rosin solution through removal of the gasoline by, for example, distillation, with or without direct steam, the as gasoline being recovered for reuse.

The refined rosin obtained by the method as illustrated above, amounts to 52% of th original. rosin, will grade K in color an 7' will give'a soap which will show practically no no discoloration on aging.

The phenol has some solvent power on' rosin, hence the separated phenol contains some rosin in addition toflthe color bodies, as

has been indicated, which rosin maybe recovered as low grade rosin by distilling oil the phenol, or as a higher grade rosin by extractin the solution with gasoline. The recovere rosin may be refined by dissolving in gasoline and extracting with phenol as iop The phenol is ratures.

described above, thus converting a portion of it into high grade rosin. 1

The process embodying my invention may be applied to the refining-or purifying of 5 low grade gum rosins for the production of high grade gum rosins and may likewise be applied to the refining of wood rosin and of rosin as .contained in drop liquor where the concentration of rosin in the drop liquor 3,0 is not too high, the best results being obtainable where t e concentration of rosin is no over about 8%. I e

In carrying out the process according to my invention the phenol may, if desired, be caused to go into solution in the rosin solvent and a homogeneous solution of resin, solvent and phenol formed, it being only necessary to have the mixture of rosin, solvent and phenol at a temperature at which the phenol will dissolve in the rosin-solution, separation of the phenol and color bodies .from the rosin solution being effected after a reduction of the temperature of the solution to a point where the major portion of thephenol will 5 be insoluble in the rosin solvent and hence will be thrown out oi solution along with the color bodies and a small proportion of the rosin. The preferred solvent for therosin is the 3'0 gasoline cut of petroleum, but it will be'understood that any light petroleum distillate.

may be used as the rosin solvent, unless. its boiling range is above that of kerosene, and it is my intention that, where in the claims appended hereto gasoline is specified, the use, as a solvent for the rosin of any operative equivalent for gasoline which is substantially immiscible with phenol, shall be included as an equivalent of gasoline Having now fully described my invention, what I claim and desire .to protect by Letters Patent is 1. The method of refining rosin, which includes dissolving rosin in a solvent normally substantially immiscible withphenohtreating the rosin solution with phenol for the extraction of color bodies from the rosin, separating phenol, and color bodies from the rosin solution and recovering refined rosin 5 from the rosin solution.

.2. The method of refining rosin, which includes dissolving rosin in a solvent, treatin the rosin solution with a' phenol normgll substantially immiscible with the solq vent for -the rosin for the extraction of color bodies from the rosin, separating phenol and color bodies from the rosin solution and recovering. refined rosin from the rosin solu 'tion.

3. The method of refining rosin, which ineludes dissolving rosin in a solvent normally substantially immiscible with phenol, treating the rosin solution with phenol for the .extraction of color bodies from the rosin,

'66 reducing the temperature'of the rosin solu-' tion, separating phenol and color bodies from the rosin solution and recovering refined rosin from the 10S1I1 solution.

4. The method of refining rosin, which includes dissolving rosin in gasoline, treating the gasoline-rosin solution with phenol for the extraction of color bodies from the rosin,

separating phenoland color bodies from the gasoline-rosin solution and recovering refined rosin from the gasoline-rosin solution.

5. The method of refining rosln, whlch includes dissolving. rosin in gasoline, treating the gasoline-rosin solution with phenol for the extraction of color bodies from the rosin, reducing the temperature of the rosin 7. In the method of refining rosin the step which includes subjecting rosin in solution in a suitablepetroleuin hydrocarbon to treatment with phenol. 8. The method of refining rosin, which includes dissolving rosin in a suitable solvent, treatin the rosin solution with a phenol capable 0 substantia-l iinmiscibility with the rosin solution and of extracting color bodies from the rosin solution, separating the phenol and-color bodies from the rosin solution and recovering refined rosin 'from the rosin solution. a

9. The method of refining rosin, whichincludes dissolving rosin in a'suitable petroleum hydrocarbon, treating the rosin solution with a phenol capable of substantial immiscibility with the rosin solution and of. extractin color bodies from the rosin solution, sepafit mg the phenol and color bodies from the rosin solution and recovering refined rosin from the rosinsolution.

i 10. The method of refining rosin, which includes dissolving resin in a suitable solvent, intimately contactingwvith-the rosin solution a phenol, capable of substantial immiscibility with the rosin solution and of extracting color bodies from the rosin solution, separating the phenol and color bodies from the rosin solution and recovering refined rosin from the rosin solution.

11. The method of refining rosin, which includes dissolving rosin in a suitable solvent, intimately contaeting yvith the rosin solution a phenol capablejqofsubstantial imniiscibility with the rosin solution and of extracting color bodies from the rosin solution, cooling the mixture, separating the. phenol and color bodies from the rosin SO lution and recovering refined rosin from the rosin solution. I

12. The method of refining rosin which includes dissolving rosin in a suitable solvent, intimately contacting phenol with the rosin solution for the extraction of color bodies from the rosin solution, se arating the phenol and color bodies from t e rosin solution and recovering refined rosin from the rosin solution.

13. The method of refining rosin, which includes dissolving rosin in a suitable solvent, intimately contacting phenol with the rosin solution forthe extraction of color bodies from the rosin solution, cooling the mixture, separating the phenol and colorbodies from the rosin solution and recovering refined rosin from the rosin solution;

-14. The method of refining rosin which includes dissolving rosin in a suitable solvent, intimately contacting with the rosin solution a phenol normally substantially immiscible with the rosin solution and capable of extracting color bodies from the rosin, separating at least a major portion of the phenol and color bodies from the rosin solution and recovering refined rosin from the rosin solution.

15. The method of refining rosin, which includes dissolving rosin in a suitable solvent, intimately contacting with the rosin solution a phenol normally substantially immiscible with the rosin solution and capable of extracting color bodies from the rosin,

cooling the mixture, separating at least a major portion of the phenol and color bodies from the rosin solution. and recovering refined rosin from the rosin solution.

In testimony of which invention, I have hereunto set my hand, at Kenvil, N. J on this 12th day of Au st, 1926.

IR W. HUMPHREY. 

